Solid-state NMR spectroscopy for the physical chemistry laboratory

Jacob J. Kinnun, Avigdor Leftin, Michael F Brown

Research output: Contribution to journalArticle

16 Citations (Scopus)

Abstract

Solid-state nuclear magnetic resonance (NMR) spectroscopy finds growing application to inorganic and organic materials, biological samples, polymers, proteins, and cellular membranes. However, this technique is often neither included in laboratory curricula nor typically covered in undergraduate courses. On the other hand, spectroscopy and molecular structure taught in second-semester undergraduate physical chemistry courses meet the minimal background prerequisites for interpreting data obtained in many solid-state NMR experiments. A solid-state 2H NMR experiment is described in which the student obtains and interprets the spectrum of a powder sample of hexamethylbenzene-d18 using a solution NMR spectrometer as found in many undergraduate institutions. A quadrupolar-echo pulse sequence is applied to the sample to obtain the 2H NMR spectrum. The spectrum of a randomly oriented powder sample consists of two spectral branches with broad shoulders. The quadrupolar frequencies corresponding to the nuclear spin transitions are interpreted in terms of molecular mobility in the solid state, that is, 3-fold rotation of the methyl groups and 6-fold rotation of the hexamethylbenzene ring. In this way, students discover that solid substances may have significant molecular motions. This undergraduate investigation employing solid-state 2H NMR provides an informative exposure to state-of-the-art research techniques by using facilities that are already in place at many undergraduate institutions. Furthermore, it demonstrates a real-life manifestation of quantum mechanics as explained in physical chemistry courses, as well as fundamentals of molecular motions such as rotation of aromatic ring compounds and methyl groups in the solid state.

Original languageEnglish (US)
Pages (from-to)123-128
Number of pages6
JournalJournal of Chemical Education
Volume90
Issue number1
DOIs
StatePublished - Jan 8 2013

Fingerprint

Physical chemistry
Nuclear magnetic resonance spectroscopy
chemistry
Nuclear magnetic resonance
experiment
Powders
mechanic
semester
Magnetic resonance spectrometers
research method
Students
Group
student
Quantum theory
curriculum
Biological materials
Curricula
Molecular structure
Polymers
Experiments

Keywords

  • Analytical Chemistry
  • Hands-On Learning/Manpulatives
  • Inquiry-Based/Discovery Learning
  • Laboratory Instruction
  • Molecular Mechanics/Dynamics
  • NMR Spectroscopy
  • Physical Chemistry
  • Solids
  • Spectroscopy
  • Upper-Division Undergraduate

ASJC Scopus subject areas

  • Chemistry(all)
  • Education

Cite this

Solid-state NMR spectroscopy for the physical chemistry laboratory. / Kinnun, Jacob J.; Leftin, Avigdor; Brown, Michael F.

In: Journal of Chemical Education, Vol. 90, No. 1, 08.01.2013, p. 123-128.

Research output: Contribution to journalArticle

Kinnun, Jacob J. ; Leftin, Avigdor ; Brown, Michael F. / Solid-state NMR spectroscopy for the physical chemistry laboratory. In: Journal of Chemical Education. 2013 ; Vol. 90, No. 1. pp. 123-128.
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